#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/32/2013296.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2013296
loop_
_publ_author_name
'Tombul, Mustafa'
'Errington, R. John'
'Coxall, Robert A.'
'Clegg, William'
_publ_section_title
;
 An alkoxide cluster with 18 Li⁺ ions encapsulating two borate
 anions, [(tBuO)₁₂Li₁₈(BO₃)₂]
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m231
_journal_page_last               m233
_journal_paper_doi               10.1107/S0108270103009636
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Li18 (B1 O3)2 (C4 H9 O1)12]'
_chemical_formula_moiety         'C48 H108 B2 Li18 O18'
_chemical_formula_sum            'C48 H108 B2 Li18 O18'
_chemical_formula_weight         1119.88
_chemical_name_systematic
;
Bis(borato)dodeca(tert-butoxo)octadecalithium
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   19.917(3)
_cell_length_b                   19.917(3)
_cell_length_c                   15.608(3)
_cell_measurement_reflns_used    1806
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.6
_cell_measurement_theta_min      2.7
_cell_volume                     5362.0(15)
_computing_cell_refinement       'local programs'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'narrow-frame ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0700
_diffrn_reflns_av_sigmaI/netI    0.0780
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6484
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         1.76
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.040
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1812
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.173
_refine_diff_density_min         -0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.1519
_refine_ls_R_factor_gt           0.0782
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0283P)²+9.227P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1526
_reflns_number_gt                1502
_reflns_number_total             2682
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            gg1167.cif
_cod_data_source_block           I
_cod_original_cell_volume        5362.0(16)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               2013296
_cod_database_fobs_code          2013296
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Li1 0.2373(3) 0.6135(3) 0.4309(3) 0.0405(11) Uani d . 1 . . Li
Li2 0.2591(3) 0.7279(3) 0.5276(3) 0.0393(11) Uani d . 1 . . Li
Li3 0.1911(3) 0.5523(3) 0.6406(3) 0.0453(12) Uani d . 1 . . Li
O1 0.26943(10) 0.71919(10) 0.40686(10) 0.0364(4) Uani d . 1 . . O
O2 0.25341(9) 0.62817(9) 0.55788(11) 0.0339(4) Uani d . 1 . . O
O3 0.21670(10) 0.47140(9) 0.62143(11) 0.0367(5) Uani d . 1 . . O
B 0.3333 0.6667 0.5611(3) 0.0308(11) Uani d S 1 . . B
C1 0.23241(15) 0.73629(15) 0.33940(17) 0.0390(6) Uani d . 1 . . C
C11 0.1508(2) 0.7138(2) 0.3664(2) 0.0736(11) Uani d . 1 . . C
H11A 0.1226 0.6590 0.3826 0.110 Uiso calc R 1 . . H
H11B 0.1241 0.7224 0.3186 0.110 Uiso calc R 1 . . H
H11C 0.1529 0.7456 0.4154 0.110 Uiso calc R 1 . . H
C12 0.22818(18) 0.68994(18) 0.26008(17) 0.0519(8) Uani d . 1 . . C
H12A 0.2807 0.7032 0.2428 0.078 Uiso calc R 1 . . H
H12B 0.2033 0.7024 0.2134 0.078 Uiso calc R 1 . . H
H12C 0.1978 0.6344 0.2730 0.078 Uiso calc R 1 . . H
C13 0.2789(2) 0.82177(18) 0.3188(2) 0.0688(10) Uani d . 1 . . C
H13A 0.2811 0.8519 0.3694 0.103 Uiso calc R 1 . . H
H13B 0.2542 0.8336 0.2714 0.103 Uiso calc R 1 . . H
H13C 0.3316 0.8352 0.3021 0.103 Uiso calc R 1 . . H
C3 0.15478(16) 0.39429(15) 0.62941(17) 0.0432(7) Uani d . 1 . . C
C31 0.08583(19) 0.38415(19) 0.5769(2) 0.0701(10) Uani d . 1 . . C
H31A 0.0708 0.4216 0.5961 0.105 Uiso calc R 1 . . H
H31B 0.0422 0.3314 0.5846 0.105 Uiso calc R 1 . . H
H31C 0.1002 0.3929 0.5162 0.105 Uiso calc R 1 . . H
C32 0.1788(2) 0.33762(17) 0.5962(2) 0.0715(11) Uani d . 1 . . C
H32A 0.1937 0.3487 0.5358 0.107 Uiso calc R 1 . . H
H32B 0.1353 0.2845 0.6018 0.107 Uiso calc R 1 . . H
H32C 0.2229 0.3431 0.6296 0.107 Uiso calc R 1 . . H
C33 0.1315(2) 0.37713(19) 0.7234(2) 0.0701(10) Uani d . 1 . . C
H33A 0.1760 0.3841 0.7572 0.105 Uiso calc R 1 . . H
H33B 0.0889 0.3236 0.7292 0.105 Uiso calc R 1 . . H
H33C 0.1145 0.4127 0.7443 0.105 Uiso calc R 1 . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Li1 O1 . 2_665 133.2(3) yes
O1 Li1 O2 . . 95.3(2) yes
O1 Li1 O2 2_665 . 101.5(2) yes
O1 Li2 O2 . . 95.7(2) yes
O1 Li2 O2 . 3_565 94.38(19) yes
O1 Li2 O3 . 3_565 150.2(3) yes
O2 Li2 O2 . 3_565 69.44(16) yes
O2 Li2 O3 . 3_565 114.1(2) yes
O2 Li2 O3 3_565 3_565 94.96(19) yes
O2 Li3 O3 . . 102.5(2) yes
O2 Li3 O3 . 14_456 111.4(2) yes
O3 Li3 O3 . 14_456 145.8(3) yes
Li1 O1 Li1 . 3_565 98.4(3) ?
Li1 O1 Li2 . . 85.1(2) ?
Li1 O1 Li2 3_565 . 84.9(2) ?
Li1 O1 C1 . . 118.9(2) ?
Li1 O1 C1 3_565 . 129.6(2) ?
Li2 O1 C1 . . 128.0(2) ?
Li1 O2 Li2 . . 80.52(18) ?
Li1 O2 Li2 . 2_665 75.17(17) ?
Li1 O2 Li3 . . 124.2(2) ?
Li1 O2 B . . 100.0(2) ?
Li2 O2 Li2 . 2_665 151.4(2) ?
Li2 O2 Li3 . . 130.1(2) ?
Li2 O2 Li3 2_665 . 77.15(18) ?
Li2 O2 B . . 88.85(16) ?
Li2 O2 B 2_665 . 80.84(15) ?
Li3 O2 B . . 122.0(2) ?
Li2 O3 Li3 2_665 15_556 90.9(2) ?
Li2 O3 Li3 2_665 . 84.7(2) ?
Li2 O3 C3 2_665 . 132.8(2) ?
Li3 O3 Li3 . 15_556 90.3(3) ?
Li3 O3 C3 . . 116.1(2) ?
Li3 O3 C3 15_556 . 128.0(2) ?
O2 B O2 . 3_565 119.86(3) yes
O2 B O2 3_565 2_665 119.86(3) ?
O2 B O2 . 2_665 119.86(3) ?
O1 C1 C11 . . 109.4(2) ?
O1 C1 C12 . . 109.6(2) ?
O1 C1 C13 . . 109.2(2) ?
C11 C1 C12 . . 108.7(2) ?
C11 C1 C13 . . 110.8(3) ?
C12 C1 C13 . . 109.1(2) ?
C1 C11 H11A . . 109.5 ?
C1 C11 H11B . . 109.5 ?
C1 C11 H11C . . 109.5 ?
H11A C11 H11B . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C1 C12 H12A . . 109.5 ?
C1 C12 H12B . . 109.5 ?
C1 C12 H12C . . 109.5 ?
H12A C12 H12B . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
C1 C13 H13A . . 109.5 ?
C1 C13 H13B . . 109.5 ?
C1 C13 H13C . . 109.5 ?
H13A C13 H13B . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
O3 C3 C31 . . 109.6(2) ?
O3 C3 C32 . . 110.4(2) ?
O3 C3 C33 . . 109.3(2) ?
C31 C3 C32 . . 108.4(3) ?
C31 C3 C33 . . 109.5(3) ?
C32 C3 C33 . . 109.6(3) ?
C3 C31 H31A . . 109.5 ?
C3 C31 H31B . . 109.5 ?
C3 C31 H31C . . 109.5 ?
H31A C31 H31B . . 109.5 ?
H31A C31 H31C . . 109.5 ?
H31B C31 H31C . . 109.5 ?
C3 C32 H32A . . 109.5 ?
C3 C32 H32B . . 109.5 ?
C3 C32 H32C . . 109.5 ?
H32A C32 H32B . . 109.5 ?
H32A C32 H32C . . 109.5 ?
H32B C32 H32C . . 109.5 ?
C3 C33 H33A . . 109.5 ?
C3 C33 H33B . . 109.5 ?
C3 C33 H33C . . 109.5 ?
H33A C33 H33B . . 109.5 ?
H33A C33 H33C . . 109.5 ?
H33B C33 H33C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Li1 O1 . 1.906(5) yes
Li1 O1 2_665 1.890(5) yes
Li1 O2 . 2.006(5) yes
Li2 O1 . 1.913(4) yes
Li2 O2 . 1.989(5) yes
Li2 O2 3_565 2.194(5) yes
Li2 O3 3_565 1.862(5) yes
Li3 O2 . 1.901(5) yes
Li3 O3 . 1.942(5) yes
Li3 O3 14_456 1.900(5) yes
O1 Li1 3_565 1.890(5) ?
O1 C1 . 1.421(3) yes
O2 Li2 2_665 2.194(5) ?
O2 B . 1.3799(16) yes
O3 Li2 2_665 1.862(5) ?
O3 Li3 15_556 1.900(5) ?
O3 C3 . 1.414(3) yes
B O2 3_565 1.3799(16) ?
B O2 2_665 1.3799(16) ?
C1 C11 . 1.514(4) ?
C1 C12 . 1.521(4) ?
C1 C13 . 1.511(4) ?
C11 H11A . 0.980 ?
C11 H11B . 0.980 ?
C11 H11C . 0.980 ?
C12 H12A . 0.980 ?
C12 H12B . 0.980 ?
C12 H12C . 0.980 ?
C13 H13A . 0.980 ?
C13 H13B . 0.980 ?
C13 H13C . 0.980 ?
C3 C31 . 1.524(4) ?
C3 C32 . 1.521(4) ?
C3 C33 . 1.526(4) ?
C31 H31A . 0.980 ?
C31 H31B . 0.980 ?
C31 H31C . 0.980 ?
C32 H32A . 0.980 ?
C32 H32B . 0.980 ?
C32 H32C . 0.980 ?
C33 H33A . 0.980 ?
C33 H33B . 0.980 ?
C33 H33C . 0.980 ?
